Production of oxidized carbon compounds



mm 3% 1924. LfilOJfiU m. a. MARTIN PRODUCTION OF OXIDIZED CARBQN COMPOUNDS Filed Jam 3, 1821 a ywawhoz PatentedSept. 30, 1924. I

UNITED STATES 1,510,150 PATENT- OFFICE.

RHETHERFORD B. MARTIN, OF NEW YORK, N. Y., ASSIGNOR T MINERALS SEPARA- TION NORTH AMERICAN CORPORATION, OF NEW YORK, N. Y.. A CORPORATION OF MARYLAND.

PRODUCTION OF OXIDIZED CARBON COMPOUNDS.

Application filed June 8,

To all whom it may concern Be it known that I, RHFIIHIERFORD B. MARTIN, a citizen of the United States, and a resident of the boron of Manhattan, city a and State of New YOIi, have invented certain new and useful Improvements in the Production of Oxidized Carbon Compounds, of which the following is a specification.

This invention relates to oxidized carbon io com ounds and is herein described as applie to the incomplete or artial oxidation of petroleum products with the production of various substances or compositions, es ecially such as are adapted among 0t er 1% things to serve as mineral-frothing agents. I have discovered that such substances as petroleum distillates can be readil oxidized by diluted oxygen in the form 0 air, with very accurate control of the conditions of oxidation and consequent uniformity and efficiency in the product, if the oxidation is effected in a confined space in the presence of carbonaceous material, especially if hard, such as ground coke or powdered charcoal. A test run with manganese peroxide in place of coke, and heated until pasty, yielded a product similar to the product obtained when using coke or charcoal.

Apparently when using a parafii-n gas oil as a raw material for such a roduct, the

most satisfactory product for t e froth flotation concentration of many ores is obtained by so controllin Y conditions as to obtain a product absorba le to about 65 or 70 per cent in concentrated sulphuric acid, and the description herein given ,in some detail is more particularly directed to the obtaining of such a product. Suitable condensing arrangements may be provided and it may be sometimes found advantageous to collect the somewhat more volatile portions of the product in separate condensers or collectors of a series, since the product first condensed appears to have mineral-frothing values somewhat inferior to the product carried past a first condenser but condensed readily in a second condenser. Apparently the presence of water vapor in the vaporized oil is advantageous when a mineral-frothing agent is the desired product. To obtain this result, water or steammay be introduced with the oil.

In the accompanying drawing is shown diagrammatically an apparatus which has 1921.. Serial No. 474,810.

been found suitable for carrying out the present invention. An oil such as paraffin gas 011 is fed through a valved tube or pipe 1 so that it runs in a small stream, or may even drop through the upper open end 2 of a retort 3. The retort 3 was made of ordinary 2-inch iron pipe forming a center section 4, screwed into n turned elbows 5 which formed end sections, the opening .2 being formed by screwing reducers (5 into the elbow so that the oil coming from the tube 1 dropped in through an opening -inch in diameter thus controlling the admission of air. Under these conditions, with the air pump shown at 7 which was used, it was found that the oil was satisfactorily volatilized and was oxidized to the desired degree by the incomin air when the bottom of the section 4 of the retort 3 was nearly but not quite half filled with powdered coke or powdered charcoal maintained at a suitable temperature by a burner shown diagrammatically at 8. The exit end 9 of the retort was formed of an upwardly extending pipe 10 like the pipe 3 and was found satis factory when about a foot in length and provided with a smaller exit pipe 11, say 4;- inch pipe, which was bent over at an elbow 12 and led into a retort 13 which formed a first air cooled condenser. Under these coir ditions the retort 3 was found to work satisfactorily when 7 inches long between vertical centers of the elbows 5.

It was found advisable to feed oil at a rate of 88 01' 40 cc. per minute when using coke or powdered charcoal in the retort 3. To avoid ignition of the oil at the beginning of a run the oil should be fed rather rapidly or with some water, the latter, as stated above, sometimes being advantageous, but when used in excessive quantities resulted in the production of an emulsion in the condensing vessels which was very difficult to separate. To observe temperatures a pyrometer 14 was inserted in the vertical section 10 of the retort and extended Substantially down to the upper end of the exit end elbow 5. This pyrometer showed that the best product for use as a mineral-frothing agent was obtained from a coke filled retort when the temperature was about 400 C. and from a charcoal filled retort when the temperature was about 350 C. It was noted that the temperature shown by the pyrometer was considerably higher. when oil was being drawn through the retort than when air alone was being drawn through. To insure uniformity of heating, the retort 3 was placed in a loose brickwork 26 and in operation was usually heated by a Bunsen burner.

The product which passed on in vapor form through the condensing retort 13 was carried by a tube or pipe 15 to a twin-necked condensing bottle 16 provided with a return condenser 17 at its exit end, which'in turn was connected by a tube 18 to a second twinnecked bottle 19 provided with a. scrubbing return condenser 20. From the scrubber 20 a tube 21 carried the still volatile parts of the product to an air pump 7, shown diagrammatically as a fan, which was connected by an exit pipe 22 to a species of filter pump 23, so that the effluent gases were absorbed by water coming fi m a tap 24 which fed the filter pump. The water containing the gases could be observed in the sink 25. It was found that the best mineral-frothing agent was collected in the condenser 16 and to a less extent in the condenser 17 when effiuent water in the sink had a very uniform frothy appearance as it ran to waste.

It was found that the oily product col lected in the receivers 16 and 19 under some conditions amounted to about 100 per cent of the oil used, over and above the water which condensed with the product. According to one analysis the escaping gases contained 4 per cent CO 2.5 per cent 0 1.1 per cent CO, and 1.6 per cent H The condensed oily product floated upon the condensed water and was separated therefrom by a clear line of demarkation. \Vhen agitating with water the frothing agent usually obtained by the above described procedure the froth produced appeared to be less dependent than are many froths upon the presence of metallic or metalliferous sulphide particles for suflic-ient persistence to allow its removal by the well known methods. In fact a froth of large and small bubbles which would last well was sometimes produced readily in the absence of sulphides or other solids. One oil used as a mineral-frothing agent and made from gas oil in the coke filled retort when used at the rate of 1.88 pounds per ton of ore yielded in a J anney machine a concentrate containing 20.53 per cent of zinc from Butte Superior zinc ore, assaying 12.74 per cent zinc, giving an extraction of 97.36 per cent. For modifying agents there were used with the oil per ton of ore 0.2 pound sulphuric acid, 0.5 pound copper sulphate and 1 pound sodium chloride.

I claim:

1. The process which consists in carrying the vapor of a carbon compound together with oxygen in a confined space across heated carbonaceous material to produce substances condensable to an oily liquid largely absorbable by concentrated sulphuric acid.

2. The process which consists in flowing an oil into contact with heated carbonaceous material in the presence of a current of air to produce substances condensable to an oily liquid largely absorbable by concentrated sulphuric acid, and collecting the product. l

3.. The process which consists in flowing a carbon compound into contact with heated hard' carbonaceous material in the presence of a current of air to produce substances condensable to an oily liquid largely absorbable by concentrated sulphuric acid, and collecting the product.

4. The process which consists in flowing a carbon compound in a gas current carrying oxygen into contact with hard carbon material heated so as to maintain during the reaction a temperature well over 200 C. above the carbonaceous material to produce substances condensable to an oily liquid largely absorbable by concentrated sulphuric acid, and collecting the product.

5. The process which consists in carrying the vapor of a carbon compound together with oxygen in a. confined space across heated hard carbonaceous material to produce substances condensable to an oily liquid largely absorbable by concentrated sulphuric acid.

6. The process which consists in flowin a petroleum distillate into contact witi heated hard carbonaceous material in the presence of a current of air to produce substances condensable to an oily liquid largely absorbable by concentrated sulphuric aci and collecting the product.

7. The process which consists in flowing a petroleum distillate into contact with heated hard carbonaceous material in the presence of a suitably regulated current of air to produce substances condensable to an oily liquid largely absorbable by concentrated sulphuric acid, and collecting the product.

8. The process which consists in flowing a petroleum distillate into contact with heated hard carbonaceous material so that the vaporized petroleum is carried in a confined space over the carbonaceous material in the presence of air to produce substances condensable to an oily liquid largely absorbable by concentrated sulphuric acid.

In testimony whereof, I have afiixed my signature to this specification.

RHETHERFORD B. MARTIN. 

